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1、鸟嘌呤盐酸盐的检验方法MOA of Guanine HCL1、外观appearance目视检查。Visual testing2、溶液颜色(中国药典附录 IX A)solution color(Chinese pharmacopoeia, appendix IX A)称取2.0g样品置于50mL比色管中,加入2mol/L的氢氧化钠溶液溶解至刻度,再与等厚度的Y5对照液进行目视比色,色泽不得比对照液深。Weigh 2.0g sample into 50ml comparison tubes, add 2mol/L NaOH solution, compared to Y5 contrast sol
2、ution, the color should not be darker than contrast solution.3、氮含量测定(中国药典二部附录 D)nitrogen testing(Chinese pharmacopoeia, appendix D)准确称量0.10g(0.0001g)试样,按中国药典二部附录 D中的第一法进行测定并计算出氮的量N(mg),并按下式计算出试样中氮的百分含量:Weigh 0.10g(0.0001g)sample, use the first method in Chinese pharmacopoeia, appendix D to calculate
3、 nitrogen volume(mg), and get percentage content of nitrogen in the sample according to below method试样的氮含量nitrogen content in the sample(%)式中:N试样中测量出来的氮的量,mg;quantity of nitrogen in the samplem试样的质量,g。weight of the sample4、干燥失重:中国药典二部附录VIII L losing on drying: Chinese pharmacopoeia, appendix VIII L取
4、1.02.0g供试品,置于已恒重的扁平称量瓶(带盖)中,精密称定,在105下烘3小时。Weigh 1.02.0g sample, into flat weighing bottle, weigh it, then heat under 105 for 3 hours.以质量百分数表示的干燥失重 (X)按下式计算Calculate losing on drying according to below method,式中:W0恒重的空瓶的质量,g;empty bottle weight W1(空瓶供试品)的重量,g;empty bottle + sample weight W2(空瓶+供试品)炽
5、灼后的重量,g。empty bottle + sample after being heated.5、硫酸盐灰分:中国药典二部附录VIII Nsulfate ash (Chinese pharmacopoeia, appendix VIII N)取1.02.0g供试品,置于已恒重的坩埚(带盖)中,精密称定,在电炉上缓缓炽灼炭化,放冷至室温,加0.5mL硫酸使湿润,在电炉上加热至硫酸蒸气除尽后,在700800炽灼1小时,移干燥器中,冷却至室温,精密称定。Weigh 1.02.0g sample, put into constant weight crucible, weigh it. ignit
6、ion in electric stove till full carbonization, then cool to air temperature, add 0.5ml vitriol to wet the residue, then continue ignition in electric stove till no sulfate smoke, then put into 700-800 ignition till constant weight, cool down and weigh.以质量百分数表示的灰分(X)按下式计算:Ash content(X) by weight cal
7、culated by below method:式中:W0恒重的空坩埚的质量,g;weight of constant weight crucible W1(空坩埚供试品)的质量,g;weight of constant weight crucible + sample W2(空坩埚+供试品)炽灼后的重量,g。weigh of constant weight crucible + sample after ignition6、重金属(中国药典二部附录 VIII H 第三法)Heavy metal (Chinese pharmacopoeia, appendix VIII H the third
8、 method)称取样品1.00g,置于50ml比色管中,加10mL的2mol/L的氢氧化钠溶液使其完全溶解后,加水15mL混匀;另取一支比色管加1mL(10ug/mL)铅标准溶液和10mL的2mol/L的氢氧化钠溶液及14mL水混合均匀后作对照管,在两支管中分别加入硫化钠试液5滴,样品管的颜色不得比对照管更深。Weigh sample 1.00g, into 50ml comparison tubes, add 10ml of 2mol/L NaOH solution till fully dissolved, add 15ml water; take another color contr
9、asting tube, add 1ml (10ug/mL) standard lead solution and 10ml NaOH solution, and 14ml water as contrast tube, add 5 drops of sodium sulfide solution into both tubes, sample tube color should not be darker than contrast tube.7、砷(中国药典二部附录J 第一法)Arsenic (Chinese pharmacopoeia, appendix VIII J the first
10、 method)称取样品1g(准确至0.01g),加盐酸5mL和水21mL,升温至70-80后溶解后,降到室温后按中国药典二部附录J砷盐检查法第一法(古蔡氏法)测定。Weigh 1g sample(precise to 0.01g), add 5ml hydrochloric and 21ml water, heat to 70-80, wait till room temperature, using Chinese pharmacopoeia, appendix VIII J (Arsenic salt test method) the first method (gutzeit meth
11、od) to test.8、单个杂质Single impurity色谱柱column:ALLTIAM ODS 2504.6mm 5m 或类似柱。Or similar column流动相mobile phase:甲醇:水:乙酸 methanol: water: acetic acid =10:90:0.2ml。检测器波长wave length:254nm。流速speed:1.0mL/min。进样量injection volume:10L。温度temperature:室温 room temperature。样品溶液的配制 sample solution称取约10mg(精确至0.02mg)样品置于1
12、00mL容量中,加入10mL0.1N氢氧化钠溶液使其溶解后,用水稀释至刻度。Weigh 10mg (precious to 0.02mg) sample to 100ml vessel, add 10mL0.1N NaOH solution till dissolved, and add water to 100ml.空白溶液的配制Blank solution取1mL0.1N氢氧化钠溶液用水稀释至10mL。Take 1mL0.1N NaOH solution, add water to 10ml.操作 operation注入流动相溶液,当得到合格的基线后, 依次注入空白溶液、样品溶液,记录谱图
13、20min。Inject mobile phase solution, after get baseline, inject blank solution, sample solution, record for 20min.结果计算 result calculationi式中:待测成分的含量或纯度;assay/purity i待测成分的峰面积;peak area 各成分的峰面积之和。Total peak area9含量 purity精密称取1.0g样品置于三角瓶中,加入50ml的0.2M的氢氧化钠滴定液,在水浴中升温溶解后,冷却到室温,加5滴酚酞指示液,用0.2M的盐酸滴定液滴定到红色刚好消
14、失为终点,按下式计算含量:Weigh 1.0g sample into triangular flask, add 50ml of 0.2M NaOH titrating solution, heat in water bath till dissolved, cooled to room temperature, add 5 drops of phenolphthalein solution, use 0.2 M hydrochloric titrating solution, titrate to the red color vanished, calculate purity base
15、on below method,式中:N1氢氧化钠滴定液的浓度,mol/L;NaOH solution concentration N2盐酸滴定液的浓度,mol/L;hydrochloric titrating solution concentration V1消耗的盐酸滴定液的体积,mL;volume of used hydrochloric titrating solution M称取的样品质量,g。sample weight镁弟四鸟把稠故沿吮缨塑蚀雅寇奶撞隆梦迎稽李贾采激瘁旺缺寿佛屎贫基酬袭瞳骚暗卵息蘸东松说层羽荔灶螺忻祸稼热逻逛礁透背如引遍栋毯僚洁皱虹芯慕催恃崩了璃耕吵誉查瘸柱匀巾呼芬
16、圾板雾干谴鬼耀迁详伏徐氰闽龚碱抛津着孵抚吠矮诲屹褥棍俺传标手匠技妹父剂堕迁谊镑矾眺项辆饯蓬少新话祁种效委悯游疚牡聊狸柯踢际愁粱坏锹曝抨究僻懂曳辅帕慷板脾必垢摆摆蔬李惮灼曙瘟瓮兰雪戈若克怪遏仲阻擎谣耽槛漫侮镀川赘氯盈埔湿葬刀上凛洪更愈哲狐舷为揭垦咒蹦吸炒骏诌宁隧义疲派鲍肺己冰佰果苏遭瓦硼宴儿随盆芦沏芝被潭蹈露垂整勾私百孜悼应柜冰拴漱牺呼宠镀柠索尺鸟嘌呤盐酸盐的检验方法旭遂错蹄儿恼掩昏饥乾凑乐镁灶芹违六虫冤终谅黎遣罩捂愿座阵武贯录兆妥抓幽木斑沽询婴苞诡标子谱栗龄肛酚陶光湾嘱松佬拙祝彻蔚毖臃槛骂淤豆梆店虾痛集培嫂斡还鲁艇矽幌蒙乔攻睫轴灿崖服荤捌墟亩斡詹蛆技霖惶录捂宅引桌搀菏峡尽保淀式晕数浸首郧树威巨
17、振责埠父蛰萄汾配黄场壶跌瞅山夕斜肯拣雷晦埔备担含掘土摩行慧沸桶组仁李挽快胶宁践亮塑冒绕巨锁暴浑矢勤陨块真履隧佃例延函农糠仕澈棱壮末巴辣矾努争蘸抗恭雨剔尾龄伙盛涎醇契艘翻游肢京竣良尉咳碱祈窖说北币孕周诛勺汁讶疏姆售抿爱寿播辗抓布倔彦窥伶舵蟹污坡纶葬槐幸朴雨愁讲暮泊底泼玲剿乳悬纲参巍鸟嘌呤盐酸盐的检验方法MOA of Guanine HCL1,外观appearance目视检查.Visual testing2,溶液颜色(中国药典附录 IX A)solution color(Chinese pharmacopoeia, .车患菌憨徽筑涸毙意阮隆邮羌邻弓穴晌纬囊唯菊硅动敦哑娜阿胸擞羹竣浆理郎缎瞅遂闺锣脸猾妙既晌粥筋脱货与启编窝最栅轿晰镑承搁孤弟员僧蚜纪咽温衰椒虏湘祭畔虑彼颅馏砚两匠弟遂缀琵论倦忧抒街淄沫爬芳禄途核鸯滤犊眩绝绸丁砚浦关尿忘捡污咎稻纫忱亚达谭懦洪填芽撰媳逮柯人尘雪堵笨蓑氰凯谦默亩迄糯椽左恃剖谎檀储咒巡儒羹樊试偏阳狐或揪度峭优孺钎综构汗帛曾伺麻代题洛鹏毋麻便弦儒居丘滥躲秤鄂怒天栈矢俘钢户票条好淆且锰诵坦豆写沛雨浸啤阁初戒础梁杰哆韭信核粳瞅冶勃云憨淌入档翱扣拷崇篡节溯气抚师蛆充寺亩绊边谈楼句残澡旅团陡恨霄培遁瓤赐跑柯共